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Bromine → HCID 86723840、化合物

HRID 576741
ノート
印刷プレビュー

反応式

HRID 576741 の反応式
[F:1][C:2]([F:18])([F:17])[C:3]1[CH:4]=[C:5]([N:9]2[CH2:14][CH2:13][C:12](=[O:15])[NH:11][C:10]2=[O:16])[CH:6]=[CH:7][CH:8]=1.BrBr.S([O-])([O-])(=O)=S.[Na+].[Na+].[Br:28][C:29]1[C:30](=[O:46])[NH:31][C:32](=[O:45])[N:33]([C:35]2[CH:40]=[CH:39][CH:38]=[C:37]([C:41]([F:44])([F:43])[F:42])[CH:36]=2)[CH:34]=1.BrC1(Br)CN(C2C=CC=C(C(F)(F)F)C=2)C(=O)NC1=O.BrC1CN(C2C=CC=C(C(F)(F)F)C=2)C(=O)NC1=O.[Cl-].[Li+]>C(O)(=O)C.CN(C)C=O.O>[Br:28][C:29]1[C:30](=[O:46])[NH:31][C:32](=[O:45])[N:33]([C:35]2[CH:40]=[CH:39][CH:38]=[C:37]([C:41]([F:44])([F:43])[F:42])[CH:36]=2)[CH:34]=1.[F:18][C:2]([F:1])([F:17])[C:3]1[CH:4]=[C:5]([N:9]2[CH:14]=[CH:13][C:12](=[O:15])[NH:11][C:10]2=[O:16])[CH:6]=[CH:7][CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

12

反応物 7

HCID 24408BromineHCID 24477Sodium ThiosulfateHCID 433294Lithium ChlorideHCID 70692250HCID 70692250、化合物HCID 86723840HCID 86723840、化合物HCID 86723842HCID 86723842、化合物HCID 86723843HCID 86723843、化合物

生成物 2

HCID 86723840HCID 86723840、化合物HCID 86723841HCID 86723841、化合物

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒HCID 962Water溶媒2 回HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 1-(3-trifluoromethylphenyl)dihydropyrimidin-2,4(1H,3H)-dione (prepared in Reference Example 96) (770.0 mg) in acetic acid (10.0 ml) was added bromine (0.18 ml) and the resulting mixture was stirred with heating under reflux for two hours. To the reaction mixture were added water (30 ml) and 10% aqueous sodium thiosulfate solution (5 ml) and the precipitated solids were collected by filtration with water to afford a mixture containing 5-bromo-1-(3-trifluoromethylphenyl)pyrimidin-2,4(1H,3H)-dione, 5,5-dibromo-1-(3-trifluoromethylphenyl)dihydropyrimidin-2,4(1H,3H)-dione and 5-bromo-1-(3-trifluoromethylphenyl)dihydropyrimidin-2,4(1H,3H)-dione (800.0 mg). A solution of the resulting mixture (800.0 mg) and lithium chloride (122.3 mg) in N,N-dimethyl formamide (5.0 ml) was stirred at 120° C. for one and a half hours. To the reaction mixture was added water (20 ml) and the resulting mixture was extracted with ethyl acetate (20 ml×2), and the organic layer was washed with water (20 ml×2) and saturated saline (20 ml), dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: hexane/ethyl acetate) to afford 5-bromo-1-(3-trifluoromethylphenyl)pyrimidin-2,4(1H,3H)-dione (473.1 mg) and 1-(3-trifluoromethylphenyl)pyrimidin-2,4(1H,3H)-dione (135.8 mg).

後処理

  1. temperaturewith heating
  2. temperatureunder reflux for two hours
  3. filtrationthe precipitated solids were collected by filtration with water
  4. customto afford a mixture
  5. extractionthe resulting mixture was extracted with ethyl acetate (20 ml×2)
  6. washthe organic layer was washed with water (20 ml×2) and saturated saline (20 ml)
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was purified by silica gel column chromatography (eluent: hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-7ca61d9bd7a843c98a1ea492b47c803d
出典データセット
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09040516B2

反応ノート

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